CN105838902A - Lead sulphide concentrate processing method based on self-propagating reacting - Google Patents
Lead sulphide concentrate processing method based on self-propagating reacting Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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Abstract
The invention discloses a lead sulphide concentrate processing method based on self-propagating reacting, belongs to the field of non-ferrous metallurgy and relates to a technological process for preparing lead oxide through self-propagating reacting, water leaching impurity removing, thermal alkali lead extracting and precipitating calcining. The lead sulphide concentrate processing method is characterized in that lead sulphide concentrate powder subjected to beneficiation and sodium peroxide powder are sufficiently stirred, uniformly mixed and compacted, and self-propagating reacting is conducted. After self-propagating reacting is completed, obtained products are subjected to leaching impurity removing with water serving as a leaching agent, enriching residues containing lead are subjected to lead leaching through a hot sodium hydroxide solution, and hot filtration is conducted; and hot alkaline leaching liquid containing the lead is quickly cooled to dissolve out lead hydroxide, and calcining decomposition is conducted to obtain a lead oxide product. According to the lead sulphide concentrate processing method based on self-propagating reacting, the technology is simple and easy to operate, the raw materials and equipment are common, easy to get and low in cost, the reaction process is quick and low in energy consumption and pollution, alkali liquor is recycled, and environment-friendly cleaner production of lead sulphide concentrates is achieved.
Description
Technical field
The invention belongs to Non-ferrous Metallurgy field, particularly relate to use self-propagating reaction green, quick, low
The method that lead oxide is prepared in energy consumption process concentrate of lead sulfide ore separation.
Background technology
Lead minerals raw material is divided into sulphide ore and oxide ore two kinds, and the lead minerals in sulphide ore is mainly galena
(PbS), vulcanized lead Ore refines the primary raw material of lead now.Concentrate of lead sulfide ore main component is generally w (Pb Zn)
45～75%, w (S) 15～20%, w (Fe) 2～10%, w (Zn) 2～8%, w (Si) 1～5%, w
(Cu) 0.01～1.5%, w (Ca) 0.5～2%, w (Al) 0.5～2%.Lead is extracted from concentrate of lead sulfide ore
Method mainly have two kinds, i.e. pyrometallurgical smelting of lead and wet method refining lead.At present, wet method refining lead still in conceptual phase,
Main employing Oxidation Leaching method, is served only for small-scale production, and contemporary industry produces the method almost all of lead and uses
Pyrometallurgical smelting of lead.
Pyrometallurgical smelting of lead method includes traditional baking with agglomeration-shaft smelting flow process, directly refining splicer's skill and heavy
Shallow lake smelting process, wherein first two method belongs to oxidation-reduction smelting category, and the latter is displacement reaction process.Oxidation
Reduction melting (patent application 201110219664.3) includes vulcanized lead and other sulfide in concentrate of lead sulfide ore
High-temperature oxydation generates oxide and uses suitable reducing agent (such as coke) that lead oxide is reduced into metallic lead collection
Two steps.Commonly used traditional-shaft smelting the flow process of baking with agglomeration of pyrometallurgical smelting of lead at present, this technique accounts for
The world produces more than the 85% of lead amount.This method treating capacity is big, stable production process, but there is energy consumption height, returning charge amount
Greatly, the problem such as difficulty, lead steam and leaded dust polluting environment, labor condition difference is reclaimed in sulfur dioxide trapping.
Directly lead smelting process is to utilize concentrate of lead sulfide ore rapid oxidation to release substantial amounts of heat, takes advantage of a situation in making furnace charge between each component
Completing all of metallurgical reaction, process reaction heat is fully used, and metallurgical furnace is airtight, use oxygen-enriched or
Pure oxygen smelting, output high-concentration sulfur dioxide flue gas is with antacid.Though this method improves recovery and the trapping degree of sulfur,
But equally exist the problems such as technological process dust pollution complicated, leaded, equipment is huge, investment is bigger.Along with height
The petering out of grade lead mineral resources, countries in the world are to the great attention of lead contamination and cleaning produces and circulation warp
The development of Ji, high energy consumption, the pyrometallurgical smelting of lead technology of high pollution have started to be restricted in countries in the world.Meanwhile,
One consumption carbon industry during the oxidation-reduction smelting of concentrate of lead sulfide ore, reducing can cost and the requirement pair lowering carbon emission
Lead is smelted and is proposed critical challenges, is badly in need of exploitation low energy consumption, high efficiency, environmentally friendly concentrate of lead sulfide ore smelting skill
Art.
Invention applies self-propagating reaction technology, water logging remove impurity, alkali extraction lead.Avoid existing pyrogenic process wet method
The problems such as high energy consumption, high cost, complex procedures such as high temperature that technique is brought, high pressure, peracid, self-propagating reaction
Speed is exceedingly fast, and product is stable, it is to avoid the generation of the sulfur-bearing toxic gas such as sulfur dioxide, it is achieved that cleaning is without dirty
Dye, application water carries out remove impurity, alkali extraction lead, overcomes concentrate of lead sulfide ore High Temperature High Pressure wet-leaching technique and bring
Environment, energy consumption, the problem such as equipment, there is good environmental economical profit.It is the easiest that the present invention has technique
OK, the raw materials used and common easy acquisition of equipment and cheap, energy consumption is low, green non-pollution.
Summary of the invention
The high energy consumption that the present invention seeks to solve to bring in existing wet method and pyrogenic process lead metallurgical process, high cost, height
The problem such as input, high pollution, complex process are tediously long.To this end, the present invention be open a kind of low power consuming, pollution-free,
The method processing concentrate of lead sulfide ore under the normal temperature and pressure conditions that technique is simple, with low cost.
The present invention it has been investigated that: vulcanized lead can occur self-propagating reaction after mixing with sodium peroxide after igniting,
Reaction generates plumbite, and the sulfur of-divalent is converted into sodium sulfate in self propagating high temperature reacts.Find according to above,
Present invention process application self-propagating reaction technology, makes vulcanized lead rely on self with the redox reaction of sodium peroxide
Chemical energy is carried out, it is not necessary to external offer additional-energy, it is achieved low energy consumption, efficiently quickly process concentrate of lead sulfide ore,
Avoid the generation of SOx dusty gas simultaneously, thoroughly solve the fume treatment that existing roasting technology brings dispose and
Problem of environmental pollution；Use water logging remove impurity, alkali extraction lead, technical process have more quick, cheap, efficient,
Low energy consumption, the advantage such as pollution-free.
A kind of method based on self-propagating reaction process concentrate of lead sulfide ore of the present invention is as follows:
Step one: self-propagating reaction
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 30～200 microns, excellent
Select 74 microns.Then breeze and sodium peroxide powder are thoroughly mixed uniformly, are compacted, be placed in high temperature resistant instead
Answer in container.Use the methods such as chemic ignition, combustion wave igniting, laser ignition, thermal explosion igniting or microwave igniting
In one or more ignite methods cause self-propagating reactions.React once ignite by with combustion wave form spontaneous enter
OK, it is not necessary to provide additional-energy, until reaction terminates.
Particularly, concentrate of lead sulfide ore powder and sodium peroxide mass ratio are 1:1～1:5, it is desirable to enter in dry environment
The mixing of row material and compacting operation.
PbS+Na2O2→NaxPbOy+Na2SO4
Step 2: water logging remove impurity
It is placed on step one is reacted afterproduct cooling in alkali resistance reaction vessel, soaks for leaching agent with water
Going out remove impurity, foreign ion is with ZnO2 2-、SiO3 2-、AlO2 -、Ca(OH)2Form is dissolved in leachate, lead,
Ferrum, copper precipitate the most in the form of an oxide, and leaching process is stirred continuously, and filter, filtrate A and leaded enrichment slag；
Rinsing lead oxide enrichment slag with sig water, washing liquid is incorporated to leachate；Filtrate A is miscellaneous by regulation pH precipitation
Prime element, filters, obtains liquor B and reclaim filtering residue, and then liquor B is recovered by filtration by adding sodium hydroxide
Sodium sulfate, filtrate i.e. residual hydrogen sodium oxide solution A recycles；
Leaching condition is: product and water are controlled at 1:50～1:200 (g/mL), extraction temperature by solid-to-liquid ratio
20～50 DEG C, extraction time 1～4h.Particularly, can be by controlling leaching process leachate in leaching process
PH is 9～12.
Leach dedoping step reaction equation as follows:
NaxPbOy+H2O→Pb(OH)2+NaOH
Pb(OH)2→PbO+H2O
ZnO+NaOH→Na2ZnO2(aq)+H2O
Al2O3+NaOH→NaAlO2(aq)+H2O
CaO+H2O→Ca(OH)2(aq)
SiO2+NaOH→Na2SiO3(aq)+H2O
Step 3: alkali extraction lead
Contain in leaded enrichment slag in step 2 is mainly composed of PbO, Fe2O3And CuO, use thermokalite
Liquid leaches alternative lead as leachate, and leaching process is stirred continuously, filtered while hot, and it is heavy to rinse with heat alkali liquid
Forming sediment, washing liquid is incorporated to heat alkali liquid leachate, filters, and obtains leaded filtrate filtering residue simultaneously and comes back for again leaching；
Leaching condition: alkali liquor is sodium hydroxide solution, naoh concentration controls 5～30%, extraction temperature
50～110 DEG C, extraction time 1～10h.
Thermokalite leaching process reaction equation is as follows:
PbO+NaOH+H2O→Na2Pb(OH)4
Step 4: precipitation prepares lead oxide
Leaded filtrate heated alkaline in step 3 is quickly cooled to 5～20 DEG C, lead dissolubility in alkaline solution
Reduce rapidly, separate out with Lead oxide hydrate form, to be precipitated complete after filter and separate said mixture, Lead oxide hydrate
Filtering residue obtains lead oxide product, the Strong oxdiative sodium liquor B reuse containing a small amount of lead 150～300 DEG C of calcining and decomposing
Leachate in step 3.
Residual hydrogen sodium oxide solution A also can be as the leachate in step 3.
The present invention have following a little:
1, have employed self-propagating reaction technology due to invention, make the vulcanized lead in concentrate of lead sulfide ore and sodium peroxide
There is self-propagating reaction, it is not necessary to providing additional-energy, response speed is exceedingly fast, and overcomes existing pyrogenic process wet processing
The problems such as high energy consumption, high cost, complex procedures such as the high temperature that brings, high pressure, peracid.And self-propagating reaction produces
Raw high temperature can realize heat recovery, it is achieved that concentrate of lead sulfide ore low energy consumption, Quick Pretreatment.Self-propagating
Reaction response product is stable, element sulphur is converted into sulfate, it is to avoid the sulfur-bearing toxic gas such as sulfur dioxide
Generation, it is achieved that cleanliness without any pollution.
3, the present invention uses water to be to leach cleaner, and cost is extremely low, and dust removal rate is high, and equipment requirements is low, green
Color is pollution-free.Lead oxide enriched product can be obtained after separated remove impurity, use thermokalite Selectively leaching lead, leach
Liquid impurity content is few, it is achieved efficiently leach the lead resource in concentrate of lead sulfide ore.
4, lead tolerance in concentrate of lead sulfide ore for all kinds concentrate of lead sulfide ore, and can be wanted by the technique of the present invention
Asking relatively low, the sulfide content concentrate of lead sulfide ore higher than 50% can be applied to this technique, has wide range of applications.
The present invention has simple for process, and raw materials used the most relatively common and cheap with equipment, energy consumption is extremely low, green
Pollution-free.
Accompanying drawing explanation
Fig. 1 represents the flow chart of a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction.
Detailed description of the invention
Embodiment 1
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 74 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:3 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Microwave heating method is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with
Water is that leaching agent carries out leaching remove impurity, and product and water are controlled at 1:50 (g/mL), leachate by solid-to-liquid ratio
PH is 10.5.Extraction temperature 50 DEG C, extraction time 1h.Filtering, rinse filtering residue with sig water, washing liquid is incorporated to
Leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by adding
Sodium hydroxide reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot sodium hydroxide
Solution leaches lead, and naoh concentration 25%, extraction temperature 85 DEG C, extraction time 5h, leaching process is continuous
Stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 10 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after
Filtering and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 300 DEG C of calcining and decomposing, containing few
The alkali liquor of amount lead is back to thermokalite and leaches operation.
Embodiment 2
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 38 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:4 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Thermal explosion igniting is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with water
Carrying out leaching remove impurity for leaching agent, product and water are controlled at 1:100 (g/mL), leachate by solid-to-liquid ratio
PH is 10.7.Extraction temperature 45 DEG C, extraction time 1.5h.Filtering, rinse filtering residue with sig water, washing liquid is also
Enter leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by mending
Hydro-oxidation sodium reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydroxide
Sodium solution leaches lead, and naoh concentration 10%, extraction temperature 105 DEG C, extraction time 4h, leaching process is not
Disconnected stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 15 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after
Filtering and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 275 DEG C of calcining and decomposing, containing few
The alkali liquor of amount lead is back to thermokalite and leaches operation.
Embodiment 3
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 180 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:5 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Drip type chemic ignition is used to cause self-propagating reaction.Reaction afterproduct cooling is placed on alkali resistance reaction vessel
In, carrying out leaching remove impurity with water for leaching agent, product and water control at 1:150 (g/mL) by solid-to-liquid ratio,
Leachate pH is 9.Extraction temperature 40 DEG C, extraction time 2h.Filter, rinse filtering residue, washing liquid with sig water
It is incorporated to leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is passed through
Adding sodium hydroxide and reclaim sodium sulfate, residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 5%, extraction temperature 110 DEG C, extraction time 3h, leaching process
Being stirred continuously, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary leaching
Go out.Leaded heated alkaline leaching liquid is quickly cooled to 12 DEG C, and lead separates out with Lead oxide hydrate form, to be precipitated complete
Filtering after one-tenth and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 225 DEG C of calcining and decomposing, contains
The alkali liquor having a small amount of lead is back to thermokalite and leaches operation.
Embodiment 4
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 53 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:2 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Electric heat ignition is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with water
Carrying out leaching remove impurity for leaching agent, product and water are controlled at 1:200 (g/mL), leachate by solid-to-liquid ratio
PH is 11.3.Extraction temperature 35 DEG C, extraction time 2.5h.Filtering, rinse filtering residue with sig water, washing liquid is also
Enter leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by mending
Hydro-oxidation sodium reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydroxide
Sodium solution leaches lead, and naoh concentration 10%, extraction temperature 100 DEG C, extraction time 2h, leaching process is not
Disconnected stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 6 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after mistake
Filter separates said mixture, and Lead oxide hydrate filtering residue obtains lead oxide product 175 DEG C of calcining and decomposing, containing a small amount of
The alkali liquor of lead is back to thermokalite and leaches operation.
Embodiment 5
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 62 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:1 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Combustion wave igniting is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with
Water is that leaching agent carries out leaching remove impurity, and product and water are controlled at 1:75 (g/mL), leachate by solid-to-liquid ratio
PH is 9.5.Extraction temperature 30 DEG C, extraction time 3h.Filtering, rinse filtering residue with sig water, washing liquid is incorporated to
Leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by adding
Sodium hydroxide reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot sodium hydroxide
Solution leaches lead, and naoh concentration 15%, extraction temperature 95 DEG C, extraction time 1h, leaching process is continuous
Stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 15 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after
Filtering and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 300 DEG C of calcining and decomposing, containing few
The alkali liquor of amount lead is back to thermokalite and leaches operation.
Embodiment 6
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 86 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:3.5 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Laser ignition is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with water
Carrying out leaching remove impurity for leaching agent, product and water are controlled at 1:125 (g/mL), leachate by solid-to-liquid ratio
PH is 10.Extraction temperature 25 DEG C, extraction time 3.5h.Filtering, rinse filtering residue with sig water, washing liquid is incorporated to
Leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by adding
Sodium hydroxide reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot sodium hydroxide
Solution leaches lead, and naoh concentration 20%, extraction temperature 90 DEG C, extraction time 6h, leaching process is continuous
Stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 18 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after
Filtering and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 150 DEG C of calcining and decomposing, containing few
The alkali liquor of amount lead is back to thermokalite and leaches operation.
Embodiment 7
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 200 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:4.5 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Thermal explosion igniting is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with water
Carrying out leaching remove impurity for leaching agent, product and water are controlled at 1:175 (g/mL), leachate by solid-to-liquid ratio
PH is 10.5.Extraction temperature 20 DEG C, extraction time 4h.Filtering, rinse filtering residue with sig water, washing liquid is incorporated to
Leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by adding
Sodium hydroxide reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot sodium hydroxide
Solution leaches lead, and naoh concentration 23%, extraction temperature 80 DEG C, extraction time 7h, leaching process is continuous
Stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 8 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after mistake
Filter separates said mixture, and Lead oxide hydrate filtering residue obtains lead oxide product 200 DEG C of calcining and decomposing, containing a small amount of
The alkali liquor of lead is back to thermokalite and leaches operation.
Embodiment 8
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 109 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:2.5 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Laser ignition is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with water
Carrying out leaching remove impurity for leaching agent, product and water are controlled at 1:80 (g/mL), leachate pH by solid-to-liquid ratio
It is 11.Leach temperature 40 DEG C, extraction time 2h.Filtering, rinse filtering residue with sig water, washing liquid is incorporated to leachate.
Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by adding sodium hydroxide
Reclaiming sodium sulfate, residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot sodium hydroxide solution to leach
Lead, naoh concentration 25%, extraction temperature 70 DEG C, extraction time 8h, leaching process is stirred continuously, heat
Filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.By leaded heat
Basic nature liquid is quickly cooled to 5 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after filter separate on
Stating mixture, Lead oxide hydrate filtering residue obtains lead oxide product 250 DEG C of calcining and decomposing, containing the alkali liquor of a small amount of lead
It is back to thermokalite and leaches operation.
Embodiment 9
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 120 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:1.5 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Chemic ignition is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with water
Carrying out leaching remove impurity for leaching agent, product and water are controlled at 1:130 (g/mL), leachate by solid-to-liquid ratio
PH is 11.5.Extraction temperature 45 DEG C, extraction time 2.5h.Filtering, rinse filtering residue with sig water, washing liquid is also
Enter leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by mending
Hydro-oxidation sodium reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydroxide
Sodium solution leaches lead, and naoh concentration 28%, extraction temperature 60 DEG C, extraction time 9h, leaching process is not
Disconnected stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 15 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after
Filtering and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 280 DEG C of calcining and decomposing, containing few
The alkali liquor of amount lead is back to thermokalite and leaches operation.
Embodiment 10
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, powder particle size 150 microns.By breeze
It is thoroughly mixed uniformly with sodium peroxide powder 1:3 in mass ratio, compacting, it is placed in high temperature resistant reaction vessel,
Microwave heating method is used to cause self-propagating reaction.Reaction afterproduct cooling is placed in alkali resistance reaction vessel, with
Water is that leaching agent carries out leaching remove impurity, and product and water control at 1:160 (g/mL) by solid-to-liquid ratio, leach
Liquid pH is 12.Extraction temperature 50 DEG C, extraction time 3h.Filtering, rinse filtering residue with sig water, washing liquid is also
Enter leachate.Filtrate A, by regulation pH precipitated impurities element, is recovered by filtration filtering residue, and liquor B is by mending
Hydro-oxidation sodium reclaims sodium sulfate, and residual hydrogen sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydroxide
Sodium solution leaches lead, and naoh concentration 30%, extraction temperature 50 DEG C, extraction time 10h, leaching process is not
Disconnected stirring, heat filtering, rinse precipitation with heat alkali liquid, washing liquid is incorporated to leachate, and filtering residue comes back for secondary and leaches.
Leaded heated alkaline leaching liquid is quickly cooled to 10 DEG C, lead with Lead oxide hydrate form separate out, to be precipitated complete after
Filtering and separate said mixture, Lead oxide hydrate filtering residue obtains lead oxide product 300 DEG C of calcining and decomposing, containing few
The alkali liquor of amount lead is back to thermokalite and leaches operation.
Claims (9)
1. the method processing concentrate of lead sulfide ore based on self-propagating reaction, it is characterised in that vulcanized lead and peroxidating
Self-propagating reaction can occur after sodium mixing after igniting, and reaction generates plumbite, and the sulfur of-divalent is at self-propagating
Pyroreaction is converted into sodium sulfate.
2. the method processing concentrate of lead sulfide ore based on self-propagating reaction, it is characterised in that comprise the following steps:
Step one: self-propagating reaction
Concentrate of lead sulfide ore powder after ore dressing is crushed the most after drying fine grinding, then by breeze and sodium peroxide powder
It is thoroughly mixed uniformly, compacting, it is placed in high temperature resistant reaction vessel；Use chemic ignition, burning wave point
One or more methods of igniting in the methods such as the igniting of fire, laser ignition, thermal explosion or microwave igniting cause from climing
Prolong reaction；React and will carry out so that combustion wave form is spontaneous once igniting, it is not necessary to additional-energy is provided, until instead
Should terminate；
Step 2: water logging remove impurity
It is placed on step one is reacted afterproduct cooling in alkali resistance reaction vessel, carries out for leachate with water
Leaching remove impurity, foreign ion is with ZnO2 2-、SiO3 2-、AlO2 -、Ca(OH)2Form is dissolved in solution, lead,
Ferrum, copper precipitate the most in the form of an oxide, and leaching process is stirred continuously, and filter, filtrate A and leaded enrichment slag；
Rinsing lead oxide enrichment slag with sig water, washing liquid is incorporated to leachate；Filtrate A is precipitated by regulation pH
Impurity element, filters, obtains liquor B and reclaim filtering residue, and then liquor B filters back by adding sodium hydroxide
Receiving sodium sulfate, filtrate i.e. residual hydrogen sodium oxide solution A recycles；
Step 3: alkali extraction lead
Contain in leaded enrichment slag in step 2 is mainly composed of PbO, Fe2O3And CuO, use thermokalite
Liquid leaches alternative lead as leachate, and leaching process is stirred continuously, filtered while hot, rinses with heat alkali liquid
Precipitation, washing liquid is incorporated to heat alkali liquid leachate, filters, and obtains leaded filtrate filtering residue simultaneously and comes back for again soaking
Go out；
Step 4: precipitation prepares lead oxide
Leaded filtrate heated alkaline in step 3 is quickly cooled to 5～20 DEG C, lead dissolubility in alkaline solution
Reduce rapidly, separate out with Lead oxide hydrate form, to be precipitated complete after filter and separate said mixture, hydroxide
Lead filtering residue obtains lead oxide product, the Strong oxdiative sodium liquor B containing a small amount of lead 150～300 DEG C of calcining and decomposing
The leachate being back in step 3.
3. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 2, it is characterised in that
Step one powder particle size 30～200 microns.
4. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 3, it is characterised in that
Powder particle size 74 microns.
5. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 2, it is characterised in that
Step one concentrate of lead sulfide ore powder and sodium peroxide mass ratio are 1:1～1:5.
6. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 2, it is characterised in that
Step 2, leaching condition is: product and water control at 1:50～1:200 (g/mL) by solid-to-liquid ratio, leaches
Temperature 20～50 DEG C, extraction time 1～4h.
7. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 2, it is characterised in that
Step 2 in leaching process by control leaching process leachate pH be 9～12.
8. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 2, it is characterised in that
Step 3 leaching condition: alkali liquor is sodium hydroxide solution, naoh concentration controls 5～30%, leaches temperature
Spend 50～110 DEG C, extraction time 1～10h.
9. according to a kind of method processing concentrate of lead sulfide ore based on self-propagating reaction of claim 2, it is characterised in that
Residual hydrogen sodium oxide solution A is as the leachate in step 3.
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| CN114772619A (en) * | 2022-04-19 | 2022-07-22 | 百色学院 | Method for recycling Bayer process red mud |
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